Preparation method of stable graphene colloidal dispersion liquid

A technology of olefin colloid and dispersion liquid, which is applied in the field of graphene preparation to achieve good stability, easy control of the reaction process, and small particles

Active Publication Date: 2014-07-23
WUHAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0011] In summary, there is no report on the use of dispersants to solve the problem of easy agglomeration of graphene oxide during the reduction process and thus to prepare stable graphene colloidal dispersions

Method used

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  • Preparation method of stable graphene colloidal dispersion liquid
  • Preparation method of stable graphene colloidal dispersion liquid
  • Preparation method of stable graphene colloidal dispersion liquid

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0048] A kind of preparation method of graphene dispersion liquid, comprises following processing step:

[0049] Mix 1g, 99.85wt% graphite powder with 23mL, 98wt% H 2 SO 4 Mix in a 250mL beaker and stir at room temperature for 24 hours; add 100mg, 99.0wt% NaNO to the beaker in a 40°C water bath 3 And stir for 5min to fully dissolve it. Slowly add 1500mg, 99.5wt% KMnO into the cup 4 , About 20min to complete the addition, control the reaction temperature below 5°C, and stir for 30min. Add 3 mL of distilled water to the beaker, wait for 5 minutes, then add 3 mL of distilled water, wait for 5 minutes, then add 40 mL of distilled water, and stir for 15 minutes. Stop the water bath and add 140 mL of distilled water and 10 mL of 30 wt% H to the beaker 2 o 2 Stir at room temperature for 5 min to terminate the reaction. Use a centrifuge to centrifuge at 10000r / min for 4min, wash with 5wt% HCl, and repeat twice. Then use centrifuge 8000r / min centrifuge 4min, wash three times wi...

Embodiment 2

[0051] A preparation method of a stable graphene dispersion, comprising the following processing steps:

[0052] Dissolve the graphene in Example 1 in 100mL, 99.7wt% ethanol, 70kHz ultrasound for 30min to peel and disperse, centrifuge at 12000r / min for 5min, wash with distilled water 2-3 times, and wash away residual ethanol. Disperse the precipitate in 100mL distilled water, ultrasonicate at 70kHz for 30min, and centrifuge at 10000r / min for 5min. The resulting supernatant is a dispersion of single-layer graphene with a concentration of 0.20mg / mL and containing about 12wt%. The prepared graphene dispersion has no obvious Tyndall effect, its zeta potential is -22.6mV, and the average particle diameter of graphene is 720.5nm.

Embodiment 3

[0054] A preparation method of a stable graphene colloidal dispersion, comprising the following processing steps:

[0055] Dissolve the graphene in Example 1 in 100 mL of 1-naphthoic acid of 4 mg, 98 wt %, 99.7 wt % ethanol, 70 kHz ultrasonic for 30 min to peel and disperse, centrifuge at 12000 r / min for 5 min, and wash 2 to 3 times with distilled water , Wash away residual 1-naphthoic acid and ethanol. Disperse the precipitate in 100mL distilled water, ultrasonicate at 70kHz for 30min, and centrifuge at 10,000r / min for 5min. The resulting supernatant is a colloidal dispersion with a concentration of 0.25mg / mL and containing about 25wt% single-layer graphene. The prepared stable graphene colloidal dispersion has Tyndall effect, its zeta potential is -36.2mV, and the average particle diameter of graphene is 387.3nm.

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Abstract

The invention discloses a preparation method of stable graphene colloidal dispersion liquid, and relates to the technical field of graphene preparation. The stable graphene colloidal dispersion liquid can be obtained by preparing graphene oxide via an improved Hummer's method, reducing graphene oxide and then treating the product by using a dispersing agent. The concentration of the stable graphene colloidal dispersion liquid is 0.21-0.25mg/mL and the stable graphene colloidal dispersion liquid contains 14-25wt% of single-layer graphene. The graphene colloidal dispersion liquid has Tyndall effects and has zeta potential of minus 41-minus 33mV and mean grain size of 250-400nm. The method is simple and practicable, is easy in control of the reaction process, does not have special requirements for equipment, is lower in cost, is easy to popularize and can be widely applied to the fields of nanoelectronics, sensors, nanocomposites, batteries, supercapacitors, hydrogen storage materials and the like.

Description

technical field [0001] The invention relates to the technical field of graphene preparation, in particular to the reduction of graphene oxide and the preparation method of a stable graphene colloidal dispersion. Background technique [0002] Graphene, as a new type of two-dimensional carbon nanomaterial, has attracted worldwide attention in recent years. The special nanostructure of graphene makes it have broad application prospects in fields such as nanoelectronics, sensors, nanocomposites, batteries, supercapacitors, and hydrogen storage materials. However, the lack of a controllable route to large-scale preparation of graphene has become a hindrance to the effective development and application of its potential. Like carbon nanotubes and many other nanomaterials, the most critical challenge in the mass production of graphene comes from the agglomeration of graphene itself. In the case of insufficient dispersion, the high specific surface area of ​​graphene tends to form ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B31/04C01B32/194
Inventor 李宏陈希元谢君樑黄进刘子睿
Owner WUHAN UNIV OF TECH
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